Lubricant having high film strength



Patented Feb.v 12, 1946 LUBRICANT HAVING HIGH FILM STRENGTH I John S. Yule, Chicago, 11]., assignor to The Pure 8i]:l Company, Chicago, 11]., a corporation of No Drawing. Application March 4, 1943, Serial No. 478,021

Claims. (01. ass-46.6)

superior load carrying characteristics to those disclosed in the aforesaid Whittier patent can be prepared by combining highly halogenated straight chain hydrocarbons such as those disclosed in the aforesaid Whittier patent with a sulfo-halogenated or sulfo-halogenated and phosphorized fatty body of the nature of those disclosed in an application to William A. Whittier and Joseph B. Stacker, Serial No. 353,840, now Patent No. 2,352,818. i

It is the object ofmy invention to provide a non-corrosive composition having the ability to carry high loads and to lubricate under extreme pressure conditions.

Other objects of my invention will become. apparent from the following description.

In order to prepare lubricating compositions in accordance with my invention a sulfo-halogenated fatty body or a sulfo-halogenated and phosphorized fatty body is combined with a minor portion of a stable highly halogenated aliphatic hydrocarbon. Although the sulfa-halogenated fatty body and the highly halogenated aliphatic hydrocarbon may be used without admixture with mineral oil, I prefer to compound these materials with 'a major portion of mineral oil of lubricating quality.

The sulfo-halogenated or sulfo-halogenated and phosphorized fatty body may be prepared by reacting sulfur chloride such as sulfur monochloride with animal, vegetable and marine fats,

oils and waxes under controlled conditions such as to produce a lubricant in which the sulfur,

chlorine and phosphorous are combined with the fatty body to the extent that the resulting product is stable and non-corrosive. Suitable fatty bodies which may be used are soya bean, lard, menhaden,

sperm, cotton seed and castor oils. Oils of low or intermediate unsaturation are preferred since the highly unsaturated oils such as linseed and tung oils have a tendency to polymerize and yield products inferior to those obtained from the oils of lower unsaturation.

In sulfo-halogenating the fatty body, it is advisable not to use in excess of 15% by weight of the sulfur-halide based on the weight of the fatty body used since larger amounts cause undesirable polymerization which increases the viscosity of the product and reduces its solubility in mineral oils. The minimum amount of sulfur halide which may be used will depend on the film strength of the resulting product desired. In general amounts above 5% should be used in order to obtain an appreciable improvement in the load carrying characteristics of the fatty body.

In preparing the sulfo-halogenated fatty body it is important that the temperature of reaction during the initial stages of reaction be maintained below 190 F. and preferably within the range of about to F. The reaction between sulfur halide and fatty body is strongly exothermic. Failure to maintain the tempera-' ture below the maximum level of about F. will result in loss of halogen and non-uniformity of the resulting product.

An effective method of preventing rise of temperature above the desired level is to carefully add the sulfur halide to the fatty body with continuous stirring while observing the temperature of the mixture. The rate of addition should be such that the temperature. does not substantially go above or below the range of 145 to 155 F. The temperature is maintained at this level until all the sulfur halide is thoroughly mixed with the fatty body and no further rise of temperature occurs.-

After the initial exothermic stage of the reaction is completed the temperature of the mixture is raised to approximately 250 to 300 F. and

preferably to 275 to 300 F. and held at thattemperature with constant stirring for a period of l to 4 hours. in incomplete chemical reaction between the $111- fur halide and fatty bodies with the result that the finished lubricant is corrosive.

Longer periods of heating may be resorted to although some loss of halogen may occur with Shorter heating periods may result corrosion test is satisfactory and the reaction is complete. The resultant material is then cooled and forms one of the finished constituents for my composition.

I prefer, however, to phosphorize the sulfo-halogenated fatty body at a temperature of about 220 to 230 F. by heating it with approximately .03 to 0.5% of phosphorus or with a material which yields approximately the same amount of phosphorous. The preferred phosphorizing agent is phosphorous sesquisulfide and it may be used in an amount of about .05 to 1% of the sulfochlorinated fatty body. Other phosphorous compounds may be used such as the halides, oxyhalides, sulfides, oxides and bi-elemental phosphorous compounds such as tin phosphide.

The phosphorization step is carried out with constant agitation at a temperature of 220 to 230 F. for a period of approximately hours. The resultant product should pass the copper corrosion strip test and should not fume when heated to temperatures as high as 300 F.

Sulfo-halogenated fatty bodies or sulfo-halogenated and phosphorized fatty bodies prepared in the manner just described may be blended with difilcultly hydrolizable, highly halogenated aliphatic compounds boiling above 180 C. such as hexachlorethane, heptachlorpropane and octochlorbutane in a ratio of approximately 2 parts of the sulfo-halogenated or sulfo-halogenated and phosphorized fatty body to one part of the halogenated aliphatic compound, to a ratio of 20 parts of the former to one part of the latter. It will be understood that the proportions may depart from the ratios just given but it has been found that when used within these proportions, the composition will hold the maximum load on the S. A. E. testing machine.

In blending the sulfo-halogenated or sulfohalogenated and phosphorized fatty body and the highly halogenated aliphatic compound with mineral lubricating oil I have found that maximum loads on the S. A. E. machine can be sustained by using from to 20% by weight of the fatty body base and from 1% to 5% by weight of the highly halogenated aliphatic compound, based on the weight of the mineral oil blend. The amounts of the two ingredients which may be added to mineral lubricating oil to enhance its load carrying ability may vary within wide limits depending on the mechanical parts to be lubricated. A

In order to demonstrate the improvement obtained by blending sulfo-chlorinated fatty body and highly halogenated aliphatic hydrocarbon with mineral oil, sulfo-chlorinated and phosphorized lard oil was prepared in the following manner:

83.02% by weight of lard oil (#1 lard oil was used in one batch and prime lard oil was used in a second batch) was mixed with 5.66% by weight of 200 viscosity at 100 of Gulf Coast neutral oil and a total of 11.32% by weight of sulfur monochloride was added to this mixture with constant stirring at such a rate that the exothermic heat of reaction maintained the temperature of the mixture at about 145 to 155 F. This required approximately one and one-half hours. After addition of the sulfur monochloride was completed, external heat was applied and the temperature was gradually increased to 275 to 285 F. The reaction mixture was held at 275 to 285 F. for three hours at the end of which time a polished copper strip immersed for three minutes showed no black deposits. The

mixture was cooled to 220 to 230 F. and 0.4% by weight of phosphorous sesquisulflde added. the agitation being continued. This mixture was held at 220 to 230 F. for five hours using con- 5 stant agitation. At the end of this time the lubricant base was cooled. The resulting product contained 5.26 of sulfur, 5.34% of chlorine and 0.21% of phosphorous by weight.

A series of samples were prepared using the base prepared as just described, heptachlorpropane and Gulf Coast mineral lubricating oil having a viscosity of 200 seconds Saybolt at 100 F. The blends were made to a viscosity of 85 to 95 seconds Saybolt at 210 F. S. A. E. load tests were made on the various blends as well as on blends of the mineral oil with the sulfo-chlo-' rinated and phosphorized base alone and with the mineral oil and heptachlorpropane oil alone. The results on these tests are given in the following table. The results represent the average of two or more runs. The percentage figures are in terms of weight.

. Table 7 s. a. s set Run Blend R. M.

in lbs.

18% base #2+82% GCMO. 15% base #l+86% GCM 15% base #2+86% GCMO 11% base #l+87% GCMO 11% base #2+89% GCMO 17% base #l+1% base #3+82% GCMO 17% base #2+l% base #3-l-82% GCMO 14% base #l+l% base #3+86% GCMO 14% base #2+l% base#3+86% GC-MO 10% base #l+l% base #3+89% GCMO 10% base #1+2% base #3+89% GCMO Base #1Sulfo-chlorinated' and phosphorized base made with prime lard oil.

Base #2-Sulfo-chlorinated and phosphorized base made with #1 lard oil.

Base #3Heptachlorpropane.

GCMO-Gulf Coast mineral oil.

It is evident from the figures in the table that by combining the sulfo-chlorinated and phosphorized lard oil with the heptachlorpropane a much greater improvement in load carrying ability was obtained than could be expected from the load carrying ability'of the sulfo-chlorinated and phosphorized lard oil and heptachlorpropane separately. For example whereas 11% of base #2 carried only 107.5 pounds and 3% of base #3 carried only '70 pounds, 10% of base #2 plus 3% of base #3 carried a load of 480 pounds.

By comparing the results in the table with the results in Table No- 1 of the aforesaid Whittier Patent No. 2,254,337 it will be seen that the improvementin load carrying ability of the composition is marked. In order to carry the maximum load on the S. A. E. machine using Whittier composition it was necessary to use 17.3% sulfurized and phosphorized fatty body and 5% heptachlorpropane as against 17% of sulfo-chlorinated and phosphorized fatty body plus 1% of I phorized fatty bodies which have been prepared in any manner as long as the resulting product contains a substantial amount, not less than about 2% by weight, of sulfur and of halogen in stably bound form so that the product willbricants either when used straight or emulsified in water.

I claim:

1. A lubricant having an S. A.. E. load test above 300 pounds at 1000 R. P. M. comprising a major quantity of mineral lubricating oil and a minor quantity of sulfa-chlorinated and phosphorized fatty body selected from the group consisting of animal, vegetable and marine fats, oils and waxes, which suite-chlorinated fatty body contains a substantial amount of sulfur and chlorine and will pass the copper corrosion strip test, and between 1 and 3% by weight of chlorinated aliphatic hydrocarbon boiling above 180 C. and containing in'excess of 85% by weight of chlorine, the combined amounts of the sulfochlorinated and phosphorlzed fatty body and chlorinated aliphatic hydrocarbon in the oil being between 11 and 18% by weight of the lubricant.

2. A lubricant in accordance with claim 1 in which the chlorinated hydrocarbon is selected from the group consisting of hexachlorethane, heptachlorpropane and octachlorbutane.

3. A lubricant having an S. A. E. load test above 300 pounds at 1000 R. P. M. comprising a major portion of mineral oil, a minor portion of sulfochlorinated and phosphorized lard oil containing not less than 2% by weight of sulfur and chlorine in stable chemical combination therewith, and between 1 and 3% by weight of chlorinated aliphatic hydrocarbon boiling above 180 C. and containing not less than by weight of chlorine, the combined amount of sulIo-chlorinated and phosphorized lard oil and chlorinated aliphatic hydrocarbon being not less than 11 nor more than 18% by weight of thelubricant.

4. A lubricant in accordance with claim 3 in which the sulfo-chlorinated and phosphorized lard oil contains approximately 5% by weight of sulfur and of chlorineand gives a good copper strip corrosion test.

5. A lubricant in accordance with claim 3 in which the sulfo-chlorinated and phosphorized fatty lard oil contains approximately 5.26% by weight of sulfur, 5.34% by weight of chlorine and 0.21% by weight of phosphorus.

JOHN S. YULE. 

